関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Bromide | HCID 6332 | — |
| 反応物 | 4-Amino-1,2,4-triazole | HCID 11432 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 178462842 | HCID 178462842 | — |
反応手順
A 500 ml round bottom flask equipped with an overhead stirrer was charged with 10.00 grams of 4-amino-1,2,4-triazole and 200 ml of acetonitrile. Ethyl bromide, 45 ml, 65.0 grams, was added to the vigorously stirred acetonitrile reaction mixture. The reaction was stirred for 8 days at ambient temperature at which time, thin layer chromatography showed that all of the 4-amino-1,2,4-triazole had been consumed. The resultant solution was then rotary evaporated down to leave a colorless oil which slowly crystallized. Solid material was heated to 60 C. for 5 hours under high vacuum, whereupon it melted and lost the remaining solvent and resolidified. Crystalline 1-ethyl-4-amino-1,2,4-triazolium bromide was recovered in essentially quantitative yield and high purity, 22.94 g, 117 mmoles. Melting point: 63-67° C.; DSC onset: 150° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07745635B1 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-61caf7398085455b86789c48313e7871 |
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| 出典メモ | uspto-grants-2010_06 |
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